ASTM F1581-08(2020)
(Specification)Standard Specification for Composition of Anorganic Bone for Surgical Implants
Standard Specification for Composition of Anorganic Bone for Surgical Implants
ABSTRACT
This specification covers material requirements for chemical composition of anorganic xenogeneic or allogeneic bone (apatite) intended for surgical implants. This specification specifically excludes synthetic hydroxylapatite, hydroxylapatite coatings, ceramic glasses, tribasic calcium phosphate, whitlockite, and alpha- and betatricalcium phosphate. Elemental analysis for calcium and phosphorus shall be consistent with the expected composition of the source of the biologically-derived bone mineral. X-ray diffraction analysis of the material shall be consistent with that specified for hydroxyapatite and calcium phosphate carbonate (carbonated apatite). The crystal size of the anorganic bone shall be determined from the X-ray diffraction data using the well-known Scherrer formula. The concentration of trace elements in the anorganic bone shall conform to the prescribed limit for: arsenic, cadmium, mercury, lead, and heavy metals (as lead), which may be determined by the following methods: inductively coupled plasma-mass spectroscopy (ICP-MS) or USP method and graphite furnace atomic absorption spectrophotometry. Organic content shall be measured either as total carbon or nitrogen or total protein by amino acid analyses. The carbonate content of the anorganic bone shall be determined. Functional groups shall be identified by infrared analysis. Requirements for biocompatibility and sterilization are given as well.
SCOPE
1.1 This specification covers material requirements for anorganic xenogeneic or allogeneic bone (apatite) intended for surgical implants. For a material to be called anorganic or deorganified bone, it must conform to this specification (see Appendix X1).
1.2 The biological response to apatite in soft tissue and bone has been characterized by a history of clinical use and by laboratory studies (1, 2, 3).2 Xenogeneic bone, with organic components present, has been shown to be antigenic in the human host (4) whereas the same material that has been completely deorganified has been shown to elicit no inflammatory or foreign body reactions in human clinical use (5, 6, 7).
1.3 This specification specifically excludes synthetic hydroxylapatite, hydroxylapatite coatings, ceramic glasses, tribasic calcium phosphate, whitlockite, and alpha- and beta-tricalcium phosphate.
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 Warning—Mercury has been designated by many regulatory agencies as a hazardous substance that can cause serious medical issues. Mercury, or its vapor, has been demonstrated to be hazardous to health and corrosive to materials. Use caution when handling mercury and mercury-containing products. See the applicable product Safety Data Sheet (SDS) for additional information. The potential exists that selling mercury or mercury-containing products, or both, is prohibited by local or national law. Users must determine legality of sales in their location.
1.6 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use. (See Appendix X2).
1.7 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
General Information
Relations
Standards Content (Sample)
This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: F1581 −08 (Reapproved 2020)
Standard Specification for
Composition of Anorganic Bone for Surgical Implants
This standard is issued under the fixed designation F1581; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use.
1.1 This specification covers material requirements for an-
(See Appendix X2).
organic xenogeneic or allogeneic bone (apatite) intended for
1.7 This international standard was developed in accor-
surgical implants. For a material to be called anorganic or
dance with internationally recognized principles on standard-
deorganified bone, it must conform to this specification (see
ization established in the Decision on Principles for the
Appendix X1).
Development of International Standards, Guides and Recom-
1.2 Thebiologicalresponsetoapatiteinsofttissueandbone
mendations issued by the World Trade Organization Technical
has been characterized by a history of clinical use and by
Barriers to Trade (TBT) Committee.
laboratory studies (1, 2, 3). Xenogeneic bone, with organic
components present, has been shown to be antigenic in the
2. Referenced Documents
human host (4) whereas the same material that has been
2.1 ASTM Standards:
completely deorganified has been shown to elicit no inflam-
D513 Test Methods forTotal and Dissolved Carbon Dioxide
matory or foreign body reactions in human clinical use (5, 6,
in Water
7).
D1688 Test Methods for Copper in Water
1.3 This specification specifically excludes synthetic
D2972 Test Methods for Arsenic in Water
hydroxylapatite, hydroxylapatite coatings, ceramic glasses,
D3557 Test Methods for Cadmium in Water
tribasic calcium phosphate, whitlockite, and alpha- and beta-
D3559 Test Methods for Lead in Water
tricalcium phosphate.
D3919 Practice for Measuring Trace Elements in Water by
Graphite Furnace Atomic Absorption Spectrophotometry
1.4 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this D4129 Test Method for Total and Organic Carbon in Water
by High Temperature Oxidation and by Coulometric
standard.
Detection
1.5 Warning—Mercuryhasbeendesignatedbymanyregu-
E1184 Practice for Determination of Elements by Graphite
latory agencies as a hazardous substance that can cause serious
Furnace Atomic Absorption Spectrometry
medicalissues.Mercury,oritsvapor,hasbeendemonstratedto
F748 PracticeforSelectingGenericBiologicalTestMethods
be hazardous to health and corrosive to materials. Use caution
for Materials and Devices
when handling mercury and mercury-containing products. See
F1185 Specification for Composition of Hydroxylapatite for
the applicable product Safety Data Sheet (SDS) for additional
Surgical Implants
information. The potential exists that selling mercury or
2.2 Code of Federal Regulations:
mercury-containing products, or both, is prohibited by local or
Title 21, Part 820
national law. Users must determine legality of sales in their
location.
2.3 National Formulary:
Tribasic Calcium Phosphate
1.6 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
This specification is under the jurisdiction of ASTM Committee F04 on Standards volume information, refer to the standard’s Document Summary page on
Medical and Surgical Materials and Devices and is under the direct responsibility of the ASTM website.
Subcommittee F04.13 on Ceramic Materials. AvailablefromU.S.GovernmentPrintingOfficeSuperintendentofDocuments,
Current edition approved Aug. 1, 2020. Published August 2020. Originally 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http://
approved in 1995. Last previous edition approved in 2016 as F1581 – 08 (2016). www.access.gpo.gov.
DOI: 10.1520/F1581-08R20. National Formulary 25. Available from U.S. Pharmacopeia (USP), 12601
The boldface numbers in parentheses refer to the list of references at the end of Twinbrook Pkwy., Rockville, MD 20852-1790, http://www.usp.org. Succeeding
this specification. USP editions may alternatively be referenced.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
F1581 − 08 (2020)
2.4 United States Pharmocopeia:
Element ppm, max
arsenic 3
Identification Tests for Calcium and Phosphate <191>
cadmium 5
Lead <251> mercury 5
lead 30
Mercury <261>
total heavy metals (as lead) 50
Cadmium <461>
For referee purposes, use either inductively coupled plasma/
Arsenic <211>
mass spectroscopy (ICP/MS) (12) or the USP methods <191>,
Heavy Metals <231> Method 1
<251>, <261>, <211>, <231> Method 1, <4617>; and for
Nitrogen Determination <4617>
cadmium, use either <461> or the U.S. Geological Survey
2.5 U.S. Geological Survey Method:
Method on cadmium. (See 2.4 and 2.5.) Graphite furnace
atomic absorption spectrophotometry may also be used for
Cadmium
analysis of trace elements using for arsenic (Test Methods
3. Terminology D2972), copper (Test Methods D1688), cadmium (Test Meth-
ods D3557), lead (Test Methods D3559) with 1 g anorganic
3.1 Definitions:
bone/100mLwater samples. General guides for the application
3.1.1 allogeneic, adj—derived from different individuals of
of the graphite furnace are given in Practices D3919 and
the same species.
E1184.
3.1.2 anorganic, adj—denoting tissue (for example, bone)
4.5 The maximum allowable limit of all heavy metals
from which the organic material has been totally removed.
determined as lead shall be 50 ppm as described in 2.4 or
Also referred to as deorganified, deproteinized or deprotein-
equivalent. Sample preparation shall be identical to that for
ated.
tribasic calcium phosphate as specified in the National Formu-
3.1.3 apatite, n—the mineral substance having the molecu-
lary (see 2.3), except that approximately1gof material shall
lar formula Ca (X) (PO ) where X = OH (hydroxyapatite or
10 2 4 6 be dissolved in approximately 30 mL of 5 % HCl and boiled.
hydroxylapatite), CO (carbonated apatite), F (fluorine), or Cl
4.6 It is recommended that all minor constituents such as
(chlorine) (8).
metals or oxides not detected as lead and present in concen-
3.1.4 xenogeneic, adj—derived from individuals of a
trations equal to or greater than 0.1 % be identified and
different, specified species. For example, bovine bone, when
quantified.
used as an implant material in humans, is xenogeneic.
4.7 Organic content shall be measured either as total carbon
ornitrogen(seeNote1)ortotalproteinbyaminoacidanalyses
4. Chemical Requirements
(13). For all methods, a synthetic hydroxylapatite control that
4.1 Elemental analysis for calcium and phosphorus shall be
conforms to Specification F1185 or an established National
consistent with the expected composition of the source of the
InstituteofStandardsandTechnology(NIST)standardshallbe
biologically-derived bone mineral (9).
used.The maximum allowable limit of either nitrogen, carbon,
or protein shall be within two standard deviations of the mean
4.2 An X-ray diffraction analysis of the material shall be
value established for the control.
consistent with PDF card #9-432 for hydroxyapatite (10) or
PDF card #35-180 for calcium phosphate carbonate (carbon-
NOTE1—TheKjeldahlprocessfornitrogendetermination(USP<461>)
ated apatite). Analysis of relative peak intensities shall be
is set forth by the Association of Official Analytical Chemists (14) as an
consistent with published data.
appropriate measure of proteins. Alternatively, organic material (carbon)
can be measured by the coulometric method (Test Method D4129).
4.3 The crystal size of the anorganic bone shall be deter-
Subtract from this value the carbonate content, which can be determined
mined from the X-ray diffraction data using the well-known
by Test Methods D513.
Scherrer formula (11).
4.8 The carbonate content of the anorganic bone shall be
4.4 The concentration of trace elements in the anorganic
determined. Carbonate content is typically 5 to6%in bone
bone shall be limited as follows:
mineral prior to removal of the organic phase. Residual
carbonate content remaining after processing is one means of
distinguishingbetweenthevariousprocessingmethodsutilized
6 to process bone powder into anorganic bone. Carbonate con-
United States Pharmacopeia 30. Available from U.S. Pharmacopeia (USP),
12601TwinbrookPkwy.,Rockville,MD20852-1790,http://www.usp.org.Succeed-
tent is linked to dissolution and resorba
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.